Hydrochloric Acid → 2,4-DI-Tert-butylcyclohexanol

HRID 277317

반응식

HRID 277317 반응식
[C:1]([CH:5]1[CH2:10][CH:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH2:8][CH2:7][C:6]1=[O:15])([CH3:4])([CH3:3])[CH3:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].Cl>CCOCC>[C:1]([CH:5]1[CH2:10][CH:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH2:8][CH2:7][CH:6]1[OH:15])([CH3:4])([CH3:3])[CH3:2]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 114442Cyclohexanone, 2,4-bis(1,1-dimethylethyl)-HCID 21226445Aluminium lithium hydride

생성물 1

HCID 5460322,4-DI-Tert-butylcyclohexanol수율 88.1%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

반응 조건

온도
23 °C

실험 절차

380 g of 2,4-di-tert-butylcyclohexanone (mixed isomers) in 200 ml of ether are added dropwise with vigorous stirring to a suspension of 34.3 g (903 mmol) of lithium aluminium hydride in 1800 ml of ether over 4 hours, and the batch is subsequently stirred at 23° C. for 1 hour and admixed with 500 ml of 5% hydrochloric acid by vigorous stirring. The organic phase is separated off and washed twice with 250 ml of water each time. The organic phase is dried over MgSO4, evaporated and dried under reduced pressure to leave 337.80 g (88% of theory) of 2,4-di-tert-butylcyclohexanol (mixed isomers) as colourless wax.

후처리

  1. customThe organic phase is separated off
  2. washwashed twice with 250 ml of water each time
  3. dry with materialThe organic phase is dried over MgSO4
  4. customevaporated
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-8f6d695d03b5483caacc35b13a61e400
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06355783B1

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